The synthesis of TBA-and DPA-VPI-5 has been studied in detail. Optimal synthesis conditions have been established using ternary composition diagrams for TBA-Al203-PzOs and DPA-Al203-PzO. Gel samples at different aging times have been examined using chemical analysis, X-ray diffraction, FT-IR, and solid-state NMR. Two reactions occur between H3P04 and pseudo-boehmite during gel aging. Interaction between the acid and the OH groups linking the pseudo-boehmite layers leads to the formation of an AI-0-P species in which A1 is 6-coordinated. A further reaction between the acid and the AI-O-P species results in the formation of a 4-coordinated A1 species. Because of the different aging conditions, the latter reaction begins much earlier in the TBA system than in the DPA system. The behavior of DPA in the synthesis gel is different from that of TBA. There is evidence that crystallization of VPI-5 proceedsvia a solid-state mechanism, and that nucleation in both systems occurs already during the aging of the gels.

Graphite oxide (GO) and its derivatives have been studied using 13C and 1H NMR. The 13C NMR lines at 60, 70, and 130 ppm are assigned to C-OH, C-O-C, and>CdC<groups in the bulk of the material, respectively. The>CdC<double bonds are relatively stable, while C-OH groups may condense to form C-O-C (ether) linkages. There are at least two magnetically inequivalent C-OH sites, and the structure does not necessarily possess long-range order. Water molecules interact very strongly with the structure. The results reveal a number of new structural features.

Stable van der Waals-bonded C60/benzene solvates were prepared using a novel crystallization technique. Solid-state NMR measurements on highly crystalline solvate under liquid benzene show that there is very little interaction between benzene and the C60 molecules and that the rotation of C60 at room temperature is not hindered. The magnetization transfer between benzene protons and local C60 molecules is highly inefficient. Three benzene species have been found in the solvate: two, nearly freely mobile, in wide and narrow porous structures, and the third constrained by C60 molecules in lattice defects. Premelting of deuterated benzene within the C60 solvate has been observed at Tm-10.5 K.

Niobium oxide (Nb2O5) supported on alumina (-Al2O3) prepared by impregnation was studied for hydration of ethylene oxide. The effects of niobium oxide loadings, calcination temperature and molar ratio of water to ethylene oxide (EO) on the reaction performance were investigated. The structure and acidity of the catalysts were characterized by using X-ray diffraction (XRD), differential thermal analysis (DTA)-thermogravimetric (TG) and infrared (IR) of pyridine adsorption. A durability test of niobic acid and Nb2O5/-Al2O3 catalyst was carried out over a period of 1000h. It was found that Nb2O5/-Al2O3 demonstrated very high activity and selectivity for hydration of ethylene oxide to monoethylene glycol (MEG) under mild conditions. Compared with the result of non-catalytic reactions, the conversion of ethylene oxide was increased from 34 to 99.8% on keeping monoethylene glycol selectivity almost unchanged when the hydration was carried out over 10wt.%Nb2O5/-Al2O3 catalyst. The yield of monoethylene glycol over Nb2O5/-Al2O3 was higher than that obtained over other solid acid catalysts. Moreover, the supported niobia catalyst demonstrated excellent stability and no deactivation was observed within 1000h of time-on-stream.

Three-dimensional porous chromium oxide single crystals have been prepared by aminosilylation of the surface silanols of the template, SBA-15, anchoring of dichromic acid to the grafted amine groups, thermal decomposition of inorganic and organic compounds, and removal of the silica framework with HF.